Semi-micro evaporation apparatus



Jan. 13, 1959 ww. ALLEN y 2,858,625

SEMI-MICRO EVAPORATION APPARATUS Filed June 18, 1956 3 Sheets-Sheret 1 ATTORNEYS Jan- 13, 1959 w. w.fALLEN 2,868,626

SEMI-MICRO -EVAPORATION APPARATUS Filed June 18, 195

5 Sheets-Sheet 2 INVENTOR.

wADE w. ALLEN ATTQRNEYS Jan 13, 1959 W. w. ALLEN 2,868,626

SEMI-MICRO EVAPORATION APPARATUS Filed June 18, 1956 3 Sheets-Sheet 3 INVENTOR. fwADE w. ALLEN ATTORNEYS 2,863,626 y SEMI-Miene nvAPonArroN APPARATUS Wade W. Allen, Kalamazoo Township, Kalamazoo County, Mich., assigner to The Upjohn Company, Kalamazoo, Mich., a corporation of Michigan Application June 18, 1956, Serial No. 592,127

7 Claims. (Cl. 23-259) This invention relates in general to equipment for lsimultaneously and continuously agitating a plurality of containers, controlling their temperatures, and removing a gas or vapor from within each container. More particularly, said invention relates to equipment operable with a plurality of containers, each containing a solution, for separating the solvent from the solute in each container and for removing such solvent from said containers.

In many types of laboratory work, it becomes necessary to evaporate solvents for the purpose of recovering materials dissolved therein. In various instances of analytical work, this becomes a particular problem where it is desired to handle a number of samples simultaneously, to draw the evaporated solvent into exhausting means and to retain the residual solute as a deposit in the container.

Further, in order to carry out effective and rapid evaporation, it is often necessary to heat the solutions within the containers, but to do so at a controlled rate in order to avoid deleterious effects on the solutes. Various of these functions have been performed by the equipment available in the prior art, but, insofar as I am aware, none of the previously available equipment has been able to perform all of these functions at one time or to do so efciently and effectively.

It is also evident that, while the foregoing discussion has dealt entirely with the withdrawal of a solvent from a plurality of solutions or solution samples, there `are many other instances in laboratory work where it is desired to agitate simultaneously a plurality of containers, control the temperatures of said containers, and withdraw a gas or vapor from within each of the containers, said gas or vapor being withdrawn under such conditions that its escape into the laboratory, or other space occupied by personnel, is effectively prevented.

Therefore, a principal object of the invention has been to provide apparatus which will simultaneously agitate solutions or solution samples contained within a plurality of containers and draw a gas or vapor from within each of said containers through a closed system to a point of reception or discharge.

A further object of the invention has been to provide a device, as aforesaid, which will effectively control the temperature of the several solutions or solution samples.

A further object of the invention has been to provide a device, as aforesaid, which can be readily assembled and disassembled for loading, use and unloading.-

A further object of the invention has been to provide a device, as aforesaid, which will have a minimum of moving parts.

A further object of the invention has been to provide a device, as aforesaid, wherein the agitation function is carried out from only a single connection, and wherein the withdrawal of gas or vapor is carried out from only a single connection. l

,A further object of the invention has been to provide a '2,868,626 Patented dan. 13, 1959 device, as aforesaid, which is of suiciently simple construction that it will be economical to fabricate and will have low maintenance costs.

A further object of the invention has been to provide a device, as aforesaid, which can be readily modified for use with containers of various sizes and shapes.

A further object of the invention has been to provide a device, as aforesaid, particularly adapted for the evaporation of sample solutions, in which the several samples can be heated to a carefully controlled 'temperature level during the evaporation process in order to avoid breakdown or other deleterious effects with respect to the solutes being obtained.

A further object of the invention has been to provide a device, as aforesaid, in which all of the operating parts are readily accessible for adjustment and/or repair, if and when such becomes necessary.

Other objects and purposes of this invention will become apparent to persons familiar with this type of equipment upon reading the following speciiication and eX- amining the accompanying drawings, in. which:

Figure 1 is a top plan view of an apparatus characterizing the invention.

Figure 2 is a broken, side elevation view of said apparatus.

Figure 3 is a sectional View taken along the lines III-HI of Figure 2.

Figure 4 is a sectional view taken along the line IV-IV ofFigure 2.

Figure 5 is a sectional view taken along the line V- of Figure 4.

Figure 6 is a sectional View taken along the line VI-VI of Figure 5.

Figure 7 is a sectional view taken. along the line VII-VII of Figure 3.

Figure 8 is a diagram of a circuit which may be used With said apparatus.

For purposes of convenience in description, the terms upper, lower, right, left, front7 and rear, as used herein, will have reference to the apparatus and parts associated therewith as appearing `in Figure 2. The terms, inner, outer, and derivatives thereof, will have reference to the geometric center of said apparatus and parts associated therewith. This terminology is for reference purposes only,` and is not limiting.

General description In order to meet the objects and purposes set forth above, aswell as others related thereto, I have provided an apparatus lll) (Figures 1 and 2) comprised of a housing 11, here elongated, upon which a plurality of conl tainers 12 are removably supported, and having a plenum chamber or manifold 13`(Figure 3) with which said containers communicate. On end of said housing 11 is removablysupported upon an actuating mechanism 14, which is arranged to impart a predetermined amount and pattern of movement to `said housing. The other end of said housing l1 is mounted upon a support mechanism 15, which merely supports lsaid cooperable other end and permits it to follow the motion impartedby the actuating mechanism i4. The actuating mechanism 14- and support mechanism 15' are both mounted upon a common vbase member 13.6. Said containers l2 are subjected to a source of heat exchange, as by insertion into a liquid bath contained within a tank i7, which tank is also supported upon the base member 16, between said actuating mechanism 14 and support mechanism 1S. A controllable heat exchange device 18, which may be conveniently mounted upon the housing 11, is provided for `maintaining the liquid within the tank 17 at a desired temperature.

Detailed construction As shown in Figures 1, 2 and 3, the base member 16 is preferably fabricated from a durable sheet material, such as steel, and is shaped to define a compartment 2li, in which is housed the major part of the wiring by which the device is operated, as hereinafter described in detail. A left end bracket 22, a front bracket 23, and a rear bracket 24, are mounted upon the upper surface of the base member 16, which is provided by the upper wall 25 of the compartment 21, for engaging the corresponding Walls of the tank 17.

The actuating mechanism 11.4 (Figures 2 and 4) includes a motor 26 having a vertical, upwardly extending shaft 27. Said motor is supported upon the upper ends of the support posts 28, the lower ends of which are secured to said upper wall 25 near the rightward end of the base member 16. The housing or frame of the motor 26 is preferably positioned to engage the rightward end of the tank 17 to substantially prevent endwise movement of the tank 17 with respect to the base member 16. Thus, by the brackets 22, 23 and 24, together with said motor 26, the tank 17 is held against all lateral movement with respect to the base member 16. but it can be readily removed therefrom merely by lifting upwardly.

The hub 29, which is removably secured to the upper end of the motor shaft 27, is provided with a radially extending, annular flange 31. at its upper end (Figures and 6). An adjustment plate 32 (Figure 6), having an elongated slot 33, is adjustably supported upon the upper surface of the ange 3l by means of a pair of machine screws 34, which slidably extend through said slot 33 for threaded engagement with said flange 3l.

The center line distance between said screws 34 is materially less than the lengthwise extent of the slot 33, thereby permitting substantial adjustment of the position of the plate 32 with respect to the flange 31 in direction parallel with the lengthwise extent of the slot 33 and transverse of the axis of the motor shaft 27.

on said plate 32 so that it can be moved with the plate j 32, upon proper adjustment of the screws 3d, between conditions of concentricity and substantial eccentricity with respect to the motor shaft 27, thereby constituting an adjustable crank.

The housing 11 (Figures l and 2) is, in this particular 4 embodiment, a relatively straight, glass tube 36, having an opening at one end, here the rightward end 37, thereof, and the other end being closed. Said tube 36 is provided with a plurality of integral, laterally and downwardly extending pipes 38, which are preferably clustered L near the center portion of the tube 36 and arranged for removable engagement with the containers l2 in a manner discussed in detail hereinafter. The open end 37 of the tube 36 may be connected, in a conventional manner, to a conventional evacuating device, such as the vacuum pump lll indicated schematically in Figure l.

The tube 36 (Figures 1, 2 and 5) is embraced between its open end 37 and said pipes 38 by a pair of spaced clamps 39 and 40, which clamps are mounted upon an elongated, relatively at connector element d2 by means of the machine bolts 43. A bearing 44 (Figure 5) is mounted upon the lower surface of the connector element 42 near the right the right end thereof, as by means of the machine bolts 43 which secure the clamp 40 to said element. The bearing d4 is axially perpendicular to the connector element 42 and arranged for snug, but removable, reception of the stub shaft 35.

The upper end of a T-shaped support post 45 is secured, with its crossbar 53 downwardly, by any convenient devices, such as the machine bolts 43 which engage the clamp 39, to the lower surface of the connector element 42 near the left end thereof. Thus, when said tank i7 and housing 11 are in position upon the base member 16, the post 45 will be disposed within, and spaced from the walls of, the right end of the tank 17. Said support post L is utilized in cooperation with the support mechanism l5 to support the housing lll when removed from the tank 17 and the base member 16 in a manner discussed in detail hereinafter.

rl`he support mechanism 15 (Figures 1, 2 and 3) is comprised of a relatively flat, substantially vertical plate 46, which is fabricated from a flexible material, suchv as sheet metal. Said plate 46 is preferably disposed, as in this particular embodiment, perpendicular to the lengthwise extent of the housing Ill and the upper Wall 25 of the compartment 2li, for reasons appearing hereinafter. The lower end 47 of the plate 6 is offset toward the actuating mechanism ltd and vertically slidably disposable between the left end bracket 22 and the adjacent end of the tank 17 when said tank is in operating position upon the base member E6. The upper end of the plate 46 is provided with an integral, leftwardly extending flange di), upon which the leftward end of the tube 36 is secured, by means of the clamp d@ and machine bolts 51.

Thus, the housing tilt will be normally held firmly in place with respect to the base member 16 or it can, at the will of the operator, be removed from its position of support upon the base member 16 merely by lifting said housing upwardly away from said member. Such lifting will disengage the lower end @7 of the plate d6 from between the bracket 22 and the tank f7, and will withdraw the bearing 44 from the stub shaft 35. The housing il can then be supported upon any horizontal surface, such as a table, said surface being engaged by the lower end 47 of the plate i6 and the crossbar 53 of the support post 45, as indicated in broken lines at 52 in Figure 2.

The outer ends of the pipes 33 (Figure 3) are provided with tapered, ground surfaces 54 (Figure 7), engageable with cooperating ground surfaces 55 on the containers 12. Said containers 12 and pipes 33 are both provided near their respectively engaging ends with a pair of diam'etrically disposed, integral hooks 56 and 57. Resilient means, such as springs 53, are used to connect the corresponding hooks 56 and 57 for holding the containers 12 in engagement with the pipes .33.

The heating device 18 includes a head 61., which is removably supported upon the tube 36 between the clamp 49 and the pipes 38, and preferably disposed above the tank 17 when said tank is in operating position (Figures l and 2) upon the base member E6. A heating element, indicated by the resistance 60 in Figure 8, of an appropriate, known type, is hermetically sealed into the lower end of a bent metal tube 62, referred to as the heater tube. The lower end of said tube is located adjacent to the lower ends of the containers l2, which containers are arranged in two substantially parallel rows, in this particular embodiment, on opposite sides of, and below, the tube 36. A temperature control 63, normally a thermostat, extends downwardly from the heating head 61 for controlling automatically the operation of the heating element 6b.

As shown in Figures l and 8, the motor 26 is controllably connected to a source of electrical potential through the power leads and a master switch 64. A switch-on light 68vis provided, as shown, to indicate the electrical energizing of the device. A. conductor '7l from one side of the power source is connected through a heater switch 66 to a conductor 72, which is connected through a conventional plug connection, if desired, to the heater element 60 and thence through the thermostat 63 and a conductor 73 back to the opposite side of the power source. Thus, upon closing of both the master switch 64 and the heater switch 66, operation of the heating element 60 is effected underthe control of the thermostat 63. A furtherllpilot light 69` is connected by the conductor 74 from a junction point 75 to a junction point 76 on the heater side of the thermostat 63. Thus, the pilot light 69 will indicate whenever the thermostat is closed and act as a warning to the operator if the thermostat stays in closed position for longer than a reasonable length of time.

Operation Before commencing the operation of the apparatus 10, it will normally be necessary to remove the housing 11, with its associated containers 12, from its position upon the base member 16, iniorder to place in said containers 12 the solutions or solution samples tobe evaporated. Because of the vertically sliding engagement of the support mechanism 15 with the end bracket22, and of the bearing 44 with the stub shaft 35, said removal ofthe housing 11 can be effected easily and quickly simply by lifting the housing 11 upwardly away fromthe base member 16. If the containers 12 are` already attached to the housing 11, they are easily and quickly removed by releasing one end of the springs 58 from the hooks 56 or 57 and drawing the containers 12 away from their associated pipes 38. The containers 12, having been removed from said pipes 38, are then Yfilled with the solutions or solution samples to be evaporated, `after which they are returned to their position of engagement with the pipes 38 and secured with respect `thereto by the springs 58. During this filling of the containers 12, the housing 11 will preferably be supported by the support mechanism 15 and the support post 45 on a convenient surface, as a table, as stated hereinabove.

The tank 17 is filled to a convenient level with a suitable liquid, such as water or oil, which can `be heated by the element 60 in the tube 62 for the purpose of heating the contents of the containers 12. The adjustment plate 32 is adjusted, as desired or required, to placethe stub shaft 35 thereon in the desired position of eccentricity with respect tovthe motor shaft27. The complete housing assembly, including the housing 11, the containers 12 attached thereto, the support mechanism 15, the connector element 42, and support post 45, is thenreturned to its position, as shown in Figures l and 2, so that the containers 12, lower end of the heating tube 62, the temperature control 63, and, in this particular embcdiment, the support post 45, are all disposed Within the "tank 17. A substantial portion of the containers 12, the

heater tube 62 and the temperature control 63 will be immersed in the liquid within the tank 17. The plate 46 will be re-engaged with the end bracket 22 and the bearing 44 will again receive the stub shaft 35. The vacuum pump 4l, or a similar device, is then connected in a conventional manner to the open end 37 of the tube 36.

The motor switch 64 and heater switch 66 may then be closed, thereby energizing the circuit shown in Figure 8. This results in imparting a rotary motion to the rightward end of the housing 11, due to the eccentricity of the stub shaft 35. The flexible plate 46 will bend leftwardly with each rotation of the motor 26, in a substantially simple, harmonic motion. Accordingly, all of the elements mounted upon the tube 436 between the support mechanism 15 and the open end 37 of said tube will be rotated in circles of increasing diameter from left to right. Thus, the containers 12 will be given a rotary motion within the tank 17, which will both agitate the heat controlling liquid within said tank and will cause the solution within said containers to move around the side walls thereof in a well-known manner. As soon as the heater switch 66 is closed, the switch-on light 68 will be illuminated. If the temperature within the tank 17 is below the desired level, the temperature control 63 will be closed, thereby energizing the heating element 60 and illuminating the heater light 69. When the liquid in the tank 17 has reached the proper temperature, the

rtemperature control 63 will open, thereby deenergizing periodically, if not visible through the liquid in the tank 17, `by opening the motor switch 64 and then raising the housing 11 away from the base member 16.

It Will be understood that while a given housing 11, if made of glass, as is usual, will be provided with pipes 38 of lixed sizes and, therefore, capable of use only with containers having mouths of correspondingly fixed sizes, the remainder of the apparatus can be readily used with a variety of different housings corresponding to the housing 11 and, hence, merely by providing a suitable supply of such housings, the apparatus can be used with a variety of different sizes and shapes of containers. Alternatively, said apparatus may be provided with adapter means, not shown, tting onto the surface 54 of the pipes 38 for receiving containers of other selected sizes and/ or shapes.

Although the liquid within the tank has been assumed to be for heating purposes, and the tube 62 has been `utilized to house a heating element, it will be obvious,

in view of the` foregoing, that if desired, as where an exothermic reaction is progressing in the containers simultaneously with the evaporating of the solvent, the heat- `ing element 60 may be replaced by a suitable cooling element and the liquid will `then function to cool the containers. Further, although the apparatus above described was developed primarily for evaporation pur poses, and such has been the use disclosed herein forl illustrative purposes, it will be evident from the foregoing that many uses are possible involvingsimultaneous agitation of material in a plurality of containers, `temperature control thereof, and withdrawal of a gas or vapor from within each container.

Thus, although a particular, preferred embodiment of my invention has been disclosed hereinabove for illustrative purposes, it will be understood that variations and modifications thereof, which come within the scope of such disclosure, are fully contemplated unlessl `chamber communicating with the interior of said containers, said containers being supported on said housing for movement therewith; a source of vacuum and means connecting said source to said chamber; a tank supported on said base member; a heat exchange medium within said tank and means for controlling the temperature thereof; means supporting said housing above said tank with said containers being positioned within said tank, said support means including means mounted on said base member for permitting movement of said housing and said containers with respect to said tank through a closed path about an axis substantially perpendicular to said housing; actuating means mounted on said base member and secured to said housing adjacent one end thereof for effecting such movement of said housing and said containers with respect to said tank.

2. Apparatus for simultaneously moving, and withdrawing a gas or vapor from a plurality of sealed, interconnected containers, comprising: a base member; a motor secured to said base member; actuating mechanism secured to the motor shaft; a tank removably positioned on said base member; a heat exchange liquid within said tank and means for controlling the temperature thereof; an elongated housing disposed above said base member,

said housing having an evacuable chamber therewithin; V

of said containers, said containers being immersed in said liquid and being supported on said housing for movement therewith; a vacuum source and removable means connecting said source to said chamber; support means secured to said housing adjacent the respective ends thereof, one of said support means being removably connected to said base member and permitting said housing and said containers to move with respect to said tank through a closed path about an axis substantially perpendicular to said housing, the other of said support means being removably connected to said actuating means whereby upon operation of said motor said actuating means causes said other support means to move said housing and containers with respect to said tank through said closed path.

3. An apparatus according to claim 2 wherein said means for controlling the temperature of said liquid includes a heating head secured to said housing, a heating element extending from said heating head into said liquid, and temperature responsive means including a switch extending from said heating head into said liquid.

4. An apparatus for supporting containers which includes: an elongated tubular housing defining a chamber and having a plurality of pipes extending therefrom, each of said pipes having a frusto-conical outer end and each of said pipes further having a plurality of hooks thereon adjacent said outer end; said containers having frustoconical openings for receiving the ends of said pipes; a plurality of hooks on each of said containers adjacent said openings; and resilient means connecting the hooks on said pipes to corresponding hooks on said containers for resiliently urging the ends of said pipes into the openings of said containers.

5. Apparatus for simultaneously moving, and Withdrawing a gas or vapor from, a plurality of sealed, interconnected containers, comprising: a base member; an elongated tubular housing defining an evacuable chamber and having a plurality of pipes extending therefrom, each of said pipes having a truste-conical outer end and having a plurality of hooks thereon adjacent said outer ends; said containers having frusto-conical openings for receiving the ends of said pipes; a plurality of hooks on each of said containers adjacent said openings; resilient means connecting the hooks on said pipes to corresponding hooks on said containers for resiliently urging the ends of said pipes into the openings in said containers; a source of vacuum and means connecting said source to said chamber; a tank supported on said base member; a heat exchange liquid within said tank and means for controlling the temperature thereof; means supporting said housing above said tank with said containers being positioned within said tank, said support means including means mountedon said base member for permitting movement of said housing and said containers with respect to said tank through a closed path about an axis substantially perpendicular to said housing; actuating means mounted on said base member and secured to said housing adjacent one end thereof for effecting movement of said housing and said containers.

6, Apparatus for simultaneously moving, and withdrawing a gas or vapor from, a plurality of sealed7 interconnected containers, comprising: a .base member; a housing defining an evacuable chamber; means removably connecting said containers to said housing with said chamber communicating with the interior of said containers, said containers being supported on said housing for movement therewith; a source of vacuum and means connecting said source to said chamber; a tank supported on said base member; a heat exchange liquid within said tank and means for controlling the temperature thereof; means supporting said housing above said tank with said containers being positioned within said tank, said support means including means mounted on said base member for permitting movement of said housing and said containers with respect to said tank through a closed path about an axis substantially perpendicular to said housing; a motor mounted on said base member with its shaft extending vertically; a vertically extending pin; a plate connected to said pin, said plate having an elongated slot therein and fastening means secured to said shaft and extending through said slot for securing said plate and pin to said shaft; a collar on said housing adjacent one end thereof, said collar having an opening for receiving said pin whereby said housing may be moved through said path.

7. .An apparatus according to claim 6 wherein said support means includes an upwardly extending flexible plate secured to said housing adjacent the other end thereof, said plate being removably connected to said base member.

References Cited in the le of this patent UNITED STATES PATENTS 1,542,843 Scott June 23, 1925 1,943,753 Biane et al. Jan. 16, 1934 2,401,782 Weller June 11, 1946 i OTHER REFERENCES Catalogue Modern Laboratory Appliance 90, Eimer and Amend, Fisher Scientific Co., 1942, N. Y., Pittsburgh, St. Louis, pages 906-907. 

1. APPARATUS FOR SIMULTANEOUSLY MOVING, AND WITHDRAWING A GAS OR VAPOR FROM, A PLURALITY OF SEALED, INTERCONNECTED CONTAINERS, COMPRISING: A BASE MEMBER; A HOUSING DEFINING AN EVACUABLE CHAMBER; MEANS REMOVABLY CONNECTING SAID CONTAINERS TO SAID HOUSING WITH SAID CHAMBER COMMUNICATING WITH THE INTERIOR OF SAID CONTAINERS, SAID CONTAINERS BEING SUPPORTED ON SAID HOUSING FOR MOVEMENT THEREWITH; A SOURCE OF VACUUM AND MEANS CONNECTING SAID SOURCE TO SAID CHAMBER; A TANK SUPPORTED ON SAID BASE MEMBER; A HEAT EXCHANGE MEDIUM WITHIN SAID TANK AND MEANS FOR CONTROLLING THE TEMPERATURE THEREOF; MEANS SUPPORTING SAID HOUSING ABOVE SAID TANK WITH SAID CONTAINERS BEING POSITIONED WITHIN SAID TANK, SAID SUPPORT MEANS INCLUDING MEANS MOUNTED ON SAID BASE MEMBER FOR PERMITTING MOVEMENT OF SAID HOUSING AND SAID CONTAINERS WITH RESPECT TO SAID TANK THROUGH A CLOSED PATH ABOUT AN AXIS SUBSTANTIALLY PERPENDICULAR TO SAID HOUSING; ACTUATING MEANS MOUNTED ON SAID BASE MEMBER AND SECURED TO SAID HOUSING ADJACENT ONE END THEREOF FOR EFFECTING SUCH MOVEMENT OF SAID HOUSING AND SAID CONTAINERS WITH RESPECT TO SAID TANK. 